Help!? Trouble in 2nd re-base using 'Pictorial Guide to Caapi Vine Alkaloid Extraction'

[Volvox]

Sorry if this is not the right place to post this. Wanted to add to the 'Pictorial Guide to Caapi Vine Alkaloid Extraction' thread but forum wouldn't let me or I couldn't find the button!


Problem - trying a 100gram cappi extraction using 'Pictorial Guide to Caapi Vine Alkaloid Extraction' tech.

Boild - got my liquid. Added NAOH base, got it to precip out. Did my acid wash with 50ml of viniger + 250ml water. and the alkaloids all dissolved in the water nicely and I removed the gunk at the bottom. My acidified water is very black. I added NAOH and brought the ph all the way back up to 12 but I can't get the alkaloids to precipitate back out! they are stuck in the liquid and refuse to come out. Tried warming the solution and boiling off then the fridge. Nothing. its stuck in the water.
Any ideas?

any advice appreciated!

 

[gibran2]

So you’re saying that after the clean-up following the first basification, in spite of thoroughly cleaning the precipitated alkaloids, your acidified solution is black?

Either you didn’t clean the alkaloids well in the first step, or there’s something strange and not easily explained going on.

 

[Volvox]

Thanks gibran2-

So I would guess that I did not get it completely clean.
I gave it 1 wash after its first balsification.
I would post an image but im not savy enough to get the

thing to work!


So if I didn't get it clean enough is there anything I can do at this point do you think or should I just throw it out?
It seems very 'base' by smell (though ph only reads 9-11ish) and its very black. Its in tall thin seperater glass things, about 250ml of it. So thick black that I can put a flash light on the other side and not see any light though it.

 

[Volvox]

oh, ok.
Bottom pic- see how black it is? There is a very thin line of alkaloids riming the very bottom but it was up to the 50ml line the first time the alkaloids settled out.

And thanks for advice, is there any saving this?

 

[Volvox]

Tried freezing, but didn't think it would do anything and it didn't.
So- I'm left with a mason jar full of black liquid that is very base and no alkaloids will fall out. Should I try to re-acidify it? If so- what would be the best acid to use at this point? I would guess that vinegar would not do much?

I could also try to boil it down to a black solid? or should I just toss it and call it a loss?

 

[endlessness]

try to filter it and see if you get something, maybe you just cant see well and they are there. If its there, even if black for some reason, you should be able to clean up by redissolving, filtering, reprecipitating, etc. But make sure your NaOH or vinegar dont have something weird which could account for the blackness...

 

[Volvox]

Thank you for the advice endlessness & gibran2. Will try with some fresh pure vinegar and see what happens!